******************************************************************************** General Structure Analysis System-II Crystal Structure Refinement by Robert B. Von Dreele & Brian H. Toby Argonne National Laboratory(C), 2010 This product includes software developed by the UChicago Argonne, LLC, as Operator of Argonne National Laboratory. Please cite: B.H. Toby & R.B. Von Dreele, J. Appl. Cryst. 46, 544-549 (2013) ******************************************************************************** Least squares controls: Refinement type: analytic Hessian Maximum number of cycles: 3 Regularize hydrogens (if any): False Initial shift factor: 1.000 Phases: Phase name: Cr2WO6 ======================================================================================================================================= X-ray scattering factors: Symbol fa fb fc --------------------------------------------------------------------------------------------------- Cr+3 9.68090 7.81136 2.87603 0.11357 5.59463 0.33439 12.82880 32.87610 0.51828 O-2 3.76936 2.53342 1.91579 1.55094 15.07970 6.30430 40.34450 0.31291 0.22789 W+6 29.49360 19.37630 13.05440 5.06412 1.42755 0.10462 5.93667 11.19720 1.01074 Neutron scattering factors: Symbol isotope mass b resonant terms --------------------------------------------------------------------------------------------------- Cr+3 Nat. Abund. 51.996 0.363 O-2 Nat. Abund. 15.999 0.581 W+6 Nat. Abund. 183.850 0.475 Space Group: P 42/m n m The lattice is centrosymmetric primitive tetragonal The Laue symmetry is 4/mmm The lattice point group is 4/mmm Multiplicity of a general site is 16 The inversion center is located at 0,0,0 The equivalent positions are: ( 1) X, Y, Z ( 2) 1/2-Y, 1/2+X, 1/2+Z ( 3) -X, -Y, Z ( 4) 1/2+Y, 1/2-X, 1/2+Z ( 5) 1/2-X, 1/2+Y, 1/2+Z ( 6) -Y, -X, Z ( 7) 1/2+X, 1/2-Y, 1/2+Z ( 8) Y, X, Z Atoms: name type refine? x y z frac site sym mult I/A Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- W1 W+6 XU 0.00000 0.00000 0.00000 1.000 mmm(z) 2 I 0.01000 Cr1 Cr+3 XU 0.00000 0.00000 0.33300 1.000mm2(d001) 4 I 0.01000 O1 O-2 XU 0.30800 0.30800 0.00000 1.000mm2(xy) 4 I 0.01000 O2 O-2 XU 0.30800 0.30800 0.33300 1.000 m(+-0) 8 I 0.01000 Unit cell: a = 4.56924 b = 4.56924 c = 8.84197 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 184.602 Refine? True Spherical harmonics texture: Order:0 Phase: Cr2WO6 in histogram: PWDR Cr2WO6_T150K.dat ======================================================================================================================================= Phase fraction : 1.0000 Refine? False Extinction coeff: 0.0000 Refine? False March-Dollase PO: 1.0000 Refine? False Axis: 0 0 1 Size model : isotropic equatorial: 1.000 Refine? False LG mixing coeff.: 1.0000 Refine? False Mustrain model: isotropic equatorial: 1000.0 Refine? False LG mixing coeff.: 1.0000 Refine? False Hydrostatic/elastic strain: names : D11 D33 values: 0 0 refine: False False Histogram: PWDR Cr2WO6_T150K.dat histogram Id: 0 ======================================================================================================================================= Instrument type: Debye-Scherrer Histogram limits: 8.00 deg to 129.92 deg Sample Parameters: Goniometer omega = 0.00, chi = 0.00, phi = 0.00 name : Scale Absorption DisplaceX DisplaceY value : 4750.2201 0.0000 -5807.3570 -1786.4670 refine: True False True True Instrument Parameters: name : Azimuth Bank Lam Polariz. SH/L U V value : 0.000000 1.000000 2.406700 0.990000 0.002000 701.362600-1157.202000 refine: False False False False False False name : W X Y Z Zero value : 558.760300 0.000000 0.000000 0.000000 0.000000 refine: False False False False False Background function: chebyschev Refine? True Coefficients: 44.097 -14.700 15.053 Refinement results: --------------------------------------------------------------------------------------------------------------------------------------- Number of function calls: 7 No. of observations: 1860 No. of parameters: 16 User rejected: 0 Sp. gp. extinct: 0 Refinement time = 0.468s, 0.156s/cycle, for 3 cycles wR = 11.69%, chi**2 = 6205.85, GOF = 1.83 ---------------------------------------------------------------------------------------------------------------------------------- Variables generated by constraints name : 0::A0 0::dAx:2 0::dAx:3 value : 0.0479 -0.0094 -0.0005 sig : 0.0000 0.0010 0.0006 Phases: Result for phase: Cr2WO6 ======================================================================================================================================= Reciprocal metric tensor: names : A11 A22 A33 A12 A13 A23 values: 0.047896281 0.047896281 0.012791100 0.000000000 0.000000000 0.000000000 esds : 0.000003289 0.000000841 New unit cell: names : a b c alpha beta gamma Volume values: 4.569294 4.569294 8.841909 90.0000 90.0000 90.0000 184.605 esds : 0.000157 0.000157 0.000291 0.017 Atoms: name x y z frac Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- W1 W+6: values: 0.00000 0.00000 0.00000 1.000-0.00405 sig : 0.00363 Cr1 Cr+3: values: 0.00000 0.00000 0.33249 1.000-0.00259 sig : 0.00169 0.00271 O1 O-2: values: 0.29857 0.29857 0.00000 1.000 0.00094 sig : 0.00099 0.00099 0.00195 O2 O-2: values: 0.30750 0.30750 0.34019 1.000 0.00420 sig : 0.00056 0.00056 0.00046 0.00136 Phase: Cr2WO6 in histogram: PWDR Cr2WO6_T150K.dat ======================================================================================================================================= Final refinement RF, RF^2 = 7.09%, 4.12% on 31 reflections Durbin-Watson statistic = 0.758 Bragg intensity sum = 6.78e+04 Histogram: PWDR Cr2WO6_T150K.dat histogram Id: 0 ======================================================================================================================================= PWDR histogram weight factor = 1.000 Final refinement wR = 11.69% on 1860 observations in this histogram Other residuals: R = 8.55%, R-bkg = 8.26%, wR-bkg = 11.69% wRmin = 6.40% Instrument type: Debye-Scherrer Sample Parameters: names : Scale Absorption DisplaceX DisplaceY values: 4358.8585 0.0000 -5912.8312 -1740.0490 sig : 56.0935 145.2470 118.9057 Background function: chebyschev value : 43.97 -15.53 13.99 sig : 0.275 0.3572 0.7087 Background sums: empirical 9.08e+04, Debye 0, peaks 0, Total 9.08e+04